CN110423547A - A kind of double-component aqueous road mark paint and preparation method thereof - Google Patents
A kind of double-component aqueous road mark paint and preparation method thereof Download PDFInfo
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- CN110423547A CN110423547A CN201910728233.6A CN201910728233A CN110423547A CN 110423547 A CN110423547 A CN 110423547A CN 201910728233 A CN201910728233 A CN 201910728233A CN 110423547 A CN110423547 A CN 110423547A
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Abstract
The invention proposes a kind of double-component aqueous road mark paints, are prepared by weight by following raw material: organic fluorin modified crylic acid resin 100-150 parts, 70-120 parts of graphene oxide modified polyurethane resin, 10-20 parts of coalescing agent, 5-10 parts of levelling agent BYK-381,3-7 parts of defoaming agent and 2-5 parts of dispersing agent.Preparation method of the present invention is simple, coating obtained is water paint, with the good feature of environmental protection, low VOC emission, and coating obtained has good gloss retention, water-fast, acidproof, chemical corrosion resistance, film forming is quickly and fine and smooth uniform, has preferable intensity and mechanical property after film forming, has broad application prospects.
Description
Technical field
The present invention relates to roadmarking technical fields, and in particular to a kind of double-component aqueous road mark paint and its preparation
Method.
Background technique
With the rapid development that highway in China is built, the annual coating dosage for roadmarking construction has reached tens of
Ten thousand tons, road mark paint has formd a very big industry.In order to meet different zones, Different climate, different constructions
The requirement of environment, road mark paint gradually from single variety to it is various in style, from low-grade to top grade, from solvent type
To environment-friendly solvent-free type, develop from simple function to multifunctional direction.For example construction is sent out from hot melt type gage mark coating for convenience
Room temperature coating is put on display, develops water paint to improve the feature of environmental protection from solvent based coating.Two-component gage mark coating is a kind of incites somebody to action
The cured two kinds of substance of reaction film forming separately constitutes two kinds of ingredients of A and B, mixes two kinds of components when graticule brushing is constructed
Coating is made, brushes film forming and is formed by curing graticule.
However current gage mark coating is required to apply in the construction process and be drawn in the road surface of dry cleansing, if pavement humidity mistake
Greatly, adhesive force of the road mark paint after film forming solidifies will be seriously affected, or even after influence graticule dry and hard time and construction
The appearance of graticule finds that often the rainwater weather due to continuous several days causes graticule to be applied in the construction and market survey of many years
Work has to interrupt.In addition, bottom surface high temperature and the bottom surface in winter that bear summer are low since graticule will bear rolling for vehicle
Often there is the phenomenon that cracking falls off or deforms in summer and winter in temperature, current graticule, and reticle life is short.
Therefore, it in order to improve every service performance of graticule, needs to change the formula and preparation method of gage mark coating
Into so that being adapted to wet road surface construction, and the performance with high anti-rolling, resistant to high temperatures, low temperature resistant and anti-deformation.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of double-component aqueous road mark paint and its preparation side
Method, it is intended that providing a kind of double-component aqueous road mark paint, preparation method is simple, and coating obtained is aqueous painting
There is material the good feature of environmental protection, low VOC emission, and coating obtained to have good gloss retention, water-fast, acidproof, chemically-resistant
Corrosivity, film forming is quickly and fine and smooth uniform, has preferable intensity and mechanical property after film forming, has broad application prospects.
The present invention provides a kind of double-component aqueous road mark paint, is prepared from the following materials: organic fluorine richness third
Olefin(e) acid resin, graphene oxide modified polyurethane resin, coalescing agent, levelling agent BYK-381, defoaming agent and dispersing agent；
It is described acrylic resin modified to be prepared from the following materials: methyl methacrylate, n-butyl acrylate, acrylic acid,
The fluorine-containing polyester polysiloxane of hydroxy-ethyl acrylate, isocyanates, terminal hydroxy group, tertiary carbonic acid glycidyl ester and initiator；
The initiator is selected from peroxidized t-butyl perbenzoate, peroxidating trimethylacetic acid tertiary butyl ester, isopropyl benzene hydroperoxide, tertiary fourth
One of base hydrogen peroxide, benzoyl peroxide, lauroyl peroxide, potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate are several
Kind；
The graphene oxide modified polyurethane resin is prepared from the following materials: graphite powder, potassium peroxydisulfate, five oxidations two
Phosphorus, potassium permanganate, sulfuric acid, 3% H2O2, Silane coupling agent KH550 and polyaminoester emulsion.
As further improvement of the invention, it is prepared by weight by following raw material: organic fluorin modified crylic acid tree
100-150 parts of rouge, 70-120 parts of graphene oxide modified polyurethane resin, 10-20 parts of coalescing agent, levelling agent BYK-381 5-
10 parts, 3-7 parts of defoaming agent and 2-5 parts of dispersing agent；
It is described acrylic resin modified to be prepared by weight by following raw material: 30-50 parts of methyl methacrylate, acrylic acid
10-30 parts of N-butyl, 20-50 parts of acrylic acid, 15-25 parts of hydroxy-ethyl acrylate, 20-30 parts of isocyanates, terminal hydroxy group are fluorine-containing poly-
5-10 parts of ester polysiloxanes, 50-100 parts of tertiary carbonic acid glycidyl ester and 1-3 parts of initiator；
The graphene oxide modified polyurethane resin is prepared by weight by following raw material: 10-20 parts of graphite powder, over cure
Sour potassium 3-6 parts, 10-20 parts of phosphorus pentoxide, 2-5 parts of potassium permanganate, 50-70 parts of sulfuric acid, 3% H2O2 10-20 parts, silane idol
Join 1-3 parts and polyaminoester emulsion 50-100 parts of agent KH550.
As further improvement of the invention, it is prepared by weight by following raw material: organic fluorin modified crylic acid tree
120-130 parts of rouge, 80-110 parts of graphene oxide modified polyurethane resin, 12-18 parts of coalescing agent, levelling agent BYK-381 6-
9 parts, 4-6 parts of defoaming agent and 3-5 parts of dispersing agent；
It is described acrylic resin modified to be prepared by weight by following raw material: 35-45 parts of methyl methacrylate, acrylic acid
15-25 parts of N-butyl, 25-45 parts of acrylic acid, 17-22 parts of hydroxy-ethyl acrylate, 20-25 parts of isocyanates, isocyanates 20-30
Part, terminal hydroxy group is polyester polysiloxane 7-9 parts fluorine-containing, 70-80 parts of tertiary carbonic acid glycidyl ester and 1-2 parts of initiator；
The graphene oxide modified polyurethane resin is prepared by weight by following raw material: 12-18 parts of graphite powder, over cure
Sour potassium 4-6 parts, 12-17 parts of phosphorus pentoxide, 3-5 parts of potassium permanganate, 55-65 parts of sulfuric acid, 3% H2O2 12-18 parts, silane idol
Join 1-2 parts and polyaminoester emulsion 70-80 parts of agent KH550.
As further improvement of the invention, it is prepared by weight by following raw material: organic fluorin modified crylic acid tree
125 parts of rouge, 95 parts of graphene oxide modified polyurethane resin, 16 parts of coalescing agent, 7 parts of levelling agent BYK-381,5 parts of defoaming agent
With 4 parts of dispersing agent；
Described acrylic resin modified to be prepared by weight by following raw material: 40 parts of methyl methacrylate, acrylic acid are just
20 parts of butyl ester, 30 parts of acrylic acid, 20 parts of hydroxy-ethyl acrylate, 25 parts of isocyanates, 8 parts of the fluorine-containing polyester polysiloxane of terminal hydroxy group,
75 parts and 1.5 parts of initiator of tertiary carbonic acid glycidyl ester；
The graphene oxide modified polyurethane resin is prepared by weight by following raw material: 16 parts of graphite powder, persulfuric acid
5 parts of potassium, 15 parts of phosphorus pentoxide, 4 parts of potassium permanganate, 60 parts of sulfuric acid, 3% H2O2 15 parts, 1.5 parts of Silane coupling agent KH550
With 75 parts of polyaminoester emulsion.
It is improved as of the invention further, described acrylic resin modified to be prepared by following methods:
S1. hydroxy-ethyl acrylate and isocyanates are dissolved in dimethylbenzene, the polymerization inhibitor for accounting for isocyanates gross mass 0.1% is added
DNBP is heated to 70 DEG C of reaction 2-3h, obtains semi-finished product；
S2. ethyl acetate is added in a kettle, oil bath heating device is warming up to 50 DEG C, tertiary carbonic acid glycidyl ester is added
Reaction kettle after mixing evenly, is added successively by monomers methyl methacrylate, n-butyl acrylate, acrylic acid adding apparatus
Semi-finished product, temperature are added the fluorine-containing polyester polysiloxane of terminal hydroxy group after rising to 70 DEG C, are stirring evenly and then adding into initiator, react 4-5h
Afterwards, solvent is removed under reduced pressure, obtains acrylic resin modified.
Preparation principle:
The hydroxyl of hydroxy-ethyl acrylate and isocyanate-reactive site reaction forming, generate semi-finished product containing double bonds, continue by
Semi-finished product are added in acrylic ester monomer and carry out polymerization reaction, obtain acrylic resin modified.Butyl acetate mixes molten with water
Agent guarantees that reaction monomers are reacted under a stable environment, avoids reaction excessively violent, improves reaction efficiency；Polymerization inhibitor is added
The purpose of agent is to prevent isocyanates autohemagglutination.By this method obtain it is acrylic resin modified have good film forming and
Weatherability, the excellent in mechanical performance after film forming.
As further improvement of the invention, the graphene oxide modified polyurethane resin is prepared by following methods:
S1. natural graphite powder, potassium peroxydisulfate and phosphorus pentoxide are weighed, is added to three mouthfuls equipped with sulfuric acid in the case of stirring
In flask, 3 h first are reacted in 60 DEG C of waters bath with thermostatic control, then three-necked flask is moved again in 25 DEG C of people of water bath with thermostatic control and reacts 5 h,
It filters, and cleans to neutrality with ionized water, dry in air, obtain pre-oxidation graphite；
S2. pre-oxidation graphite is weighed, is added in the three-necked flask equipped with sulfuric acid, is put into ice-water bath in the case of stirring,
After pre-oxidizing graphite and all dissolving, potassium permanganate is added, reacts 2 h, then three-necked flask is moved to 35 DEG C of people of water bath with thermostatic control
Middle reaction 40min, is eventually adding deionized water, continues 35 DEG C of 1 h of reaction, and 30% H is finally added dropwise2O2, so that there is no gases
Until generation, solution becomes glassy yellow, while hot centrifugal filtration, and is cleaned with a large amount of 5% hydrochloric acid and deionized water to neutrality, will
Final sediment is after the ultrasonic vibration of 1h, and dry 24 h obtain the graphite oxide of sheet at 90 DEG C in the culture dish of falling people
Alkene；
S3. the preparation of graphene oxide modified polyurethane resin: being warming up to 40 DEG C for reactor, and polyaminoester emulsion, oxidation is added
Graphene is stirring evenly and then adding into Silane coupling agent KH550, after reacting 2-3h, obtains graphene oxide modified polyurethane resin.
Improved as of the invention further, the dispersing agent be selected from hexenyl bis-stearamides, glyceryl monostearate,
Glyceryl tristearate, polycarboxylic acids ammonium salt, sodium acrylate salt copolymer, polyethylene glycol 200, polyethylene glycol 400, styrene-horse
Come one or more of acid anhydrides and CT-136.
As further improvement of the invention, the defoaming agent is selected from GPE type defoaming agent, organic silicon defoamer and BYK024
One or more of.
It is improved as of the invention further, the coalescing agent includes antioxidant, 800 mesh calcium powders, adipate ester, the third two
Alcohol block polyether, triethoxy octyl silane, Tween-80 and Arlacel-80.
The present invention further protects a kind of method for preparing above-mentioned double-component aqueous road mark paint, including following step
It is rapid: to sequentially add organic fluorin modified crylic acid resin, graphene oxide modified polyurethane resin, levelling agent BYK- by formula ratio
381, dispersing agent and defoaming agent, stir evenly；Then coalescing agent is added, is ground after mixing evenly, until reaching regulation
Fineness obtains double-component aqueous road mark paint.
The invention has the following beneficial effects:
The present invention is acrylic resin modified using organic fluorinated silicone compound and tertiary carbonic acid glycidyl ester, wherein Organic fluoride, organic
The acrylic resin of Si modification can significantly improve water-fast, the resistance to soiling of the coating of acrylic resin formation, and versatic acid shrinks sweet
Grease is the active solvent of the synthetic resin in acrylic resin, molten without adding in the acrylic resin modified synthesis
Agent improves its safety and environmental protection performance, simultaneously as the steric effect of tertiary carbonic acid glycidyl ester, so that final resin is with good
Good acid resistance improves the gloss retention of coating moreover, it is insensitive to UV；Using graphene oxide modified polyurethane resin,
The mechanical property and wear-resisting property of polyurethane resin can be significantly improved；
Paint film toughness and intensity are improved using adipate ester；It is not volatile using propylene glycol block polyether, it can dissolve in paint
Fine oxide crystallization in pigments and fillers prevents it from forming the structure reduction paint film intensity for destroying paint film；It is pungent using triethoxy
Surface of the paint film smoothness can be improved in base silane, not only promotes paint film appearance, and it is wear-resisting also to can reduce the coarse raising of surface of the paint film
Performance；The ageing-resistant performance of coating is improved using antioxidant；Adding surfactant reduces the surface tension of coating, and it is viscous to enhance it
Attached property；
Preparation method of the present invention is simple, and coating obtained is water paint, has the good feature of environmental protection, low VOC emission, and make
The coating obtained has good gloss retention, water-fast, acidproof, chemical corrosion resistance, and film forming is quickly and fine and smooth uniform, has after film forming
Preferable intensity and mechanical property, have broad application prospects.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, the embodiment described is the embodiment of part of representative of the invention, rather than whole embodiments, this field are general
Other all embodiments obtained belong to protection of the invention to logical technical staff without making creative work
Range.
Embodiment 1
Raw material form (parts by weight): 100 parts of organic fluorin modified crylic acid resin, 70 parts of graphene oxide modified polyurethane resin,
10 parts of coalescing agent, 5 parts of levelling agent BYK-381,3 parts of GPE type defoaming agent and 2 parts of glyceryl tristearate.Coalescing agent by with
Lower weight percent at being grouped as: antioxidant 6%, 800 mesh calcium powders 20%, adipate ester 14%, propylene glycol block polyether 15%, three
Ethyoxyl octyl silane 10%, Tween-80 15% and Arlacel-80 10%.
Acrylic resin modified to be prepared by weight by following raw material: 30 parts of methyl methacrylate, acrylic acid are just
10 parts of butyl ester, 20 parts of acrylic acid, 15 parts of hydroxy-ethyl acrylate, 20 parts of isocyanates, 5 parts of the fluorine-containing polyester polysiloxane of terminal hydroxy group,
50 parts and 1 part of tert-butyl hydroperoxide of tertiary carbonic acid glycidyl ester.
It is acrylic resin modified to be prepared by following methods:
S1. hydroxy-ethyl acrylate and isocyanates are dissolved in dimethylbenzene, the polymerization inhibitor for accounting for isocyanates gross mass 0.1% is added
DNBP is heated to 70 DEG C of reaction 2h, obtains semi-finished product；
S2. ethyl acetate is added in a kettle, oil bath heating device is warming up to 50 DEG C, tertiary carbonic acid glycidyl ester is added
Reaction kettle after mixing evenly, is added successively by monomers methyl methacrylate, n-butyl acrylate, acrylic acid adding apparatus
Semi-finished product, temperature are added the fluorine-containing polyester polysiloxane of terminal hydroxy group after rising to 70 DEG C, are stirring evenly and then adding into perbenzoic acid uncle
Butyl ester is removed under reduced pressure solvent, obtains acrylic resin modified after reacting 4h.
Graphene oxide modified polyurethane resin is prepared by weight by following raw material: 10 parts of graphite powder, persulfuric acid
3 parts of potassium, 10 parts of phosphorus pentoxide, 2 parts of potassium permanganate, 50 parts of sulfuric acid, 3% H2O2 10 parts, 1 part of Silane coupling agent KH550 and
50 parts of polyaminoester emulsion.
Graphene oxide modified polyurethane resin is prepared by following methods:
S1. natural graphite powder, potassium peroxydisulfate and phosphorus pentoxide are weighed, is added to three mouthfuls equipped with sulfuric acid in the case of stirring
In flask, 3 h first are reacted in 60 DEG C of waters bath with thermostatic control, then three-necked flask is moved again in 25 DEG C of people of water bath with thermostatic control and reacts 5 h,
It filters, and cleans to neutrality with ionized water, dry in air, obtain pre-oxidation graphite；
S2. pre-oxidation graphite is weighed, is added in the three-necked flask equipped with sulfuric acid, is put into ice-water bath in the case of stirring,
After pre-oxidizing graphite and all dissolving, potassium permanganate is added, reacts 2 h, then three-necked flask is moved to 35 DEG C of people of water bath with thermostatic control
Middle reaction 40min, is eventually adding deionized water, continues 35 DEG C of 1 h of reaction, and 30% H is finally added dropwise2O2, so that there is no gases
Until generation, solution becomes glassy yellow, while hot centrifugal filtration, and is cleaned with a large amount of 5% hydrochloric acid and deionized water to neutrality, will
Final sediment is after the ultrasonic vibration of 1h, and dry 24 h obtain the graphite oxide of sheet at 90 DEG C in the culture dish of falling people
Alkene；
S3. the preparation of graphene oxide modified polyurethane resin: being warming up to 40 DEG C for reactor, and polyaminoester emulsion, oxidation is added
Graphene is stirring evenly and then adding into Silane coupling agent KH550, after reacting 2h, obtains graphene oxide modified polyurethane resin.
The preparation method of double-component aqueous road mark paint, comprising the following steps: sequentially add Organic fluoride by formula ratio
Acrylic resin modified, graphene oxide modified polyurethane resin, levelling agent BYK-381, glyceryl tristearate and GPE type disappear
Infusion stirs evenly；Then coalescing agent is added, is ground after mixing evenly, until reaching regulation fineness, obtains two-component
Water-based road guide line coating.
Embodiment 2
Raw material form (parts by weight): 150 parts of organic fluorin modified crylic acid resin, 120 parts of graphene oxide modified polyurethane resin,
20 parts of coalescing agent, 10 parts of levelling agent BYK-381,7 parts of organic silicon defoamer and T-1365 parts of dispersing agent C.Coalescing agent by with
Lower weight percent at being grouped as: antioxidant 6%, 800 mesh calcium powders 20%, adipate ester 14%, propylene glycol block polyether 15%, three
Ethyoxyl octyl silane 10%, Tween-80 15% and Arlacel-80 10%.
Acrylic resin modified to be prepared by weight by following raw material: 50 parts of methyl methacrylate, acrylic acid are just
30 parts of butyl ester, 50 parts of acrylic acid, 25 parts of hydroxy-ethyl acrylate, 30 parts of isocyanates, 10 parts of the fluorine-containing polyester polysiloxane of terminal hydroxy group,
100 parts and 3 parts of sodium peroxydisulfate of tertiary carbonic acid glycidyl ester.
It is acrylic resin modified to be prepared by following methods:
S1. hydroxy-ethyl acrylate and isocyanates are dissolved in dimethylbenzene, the polymerization inhibitor for accounting for isocyanates gross mass 0.1% is added
DNBP is heated to 70 DEG C of reaction 3h, obtains semi-finished product；
S2. ethyl acetate is added in a kettle, oil bath heating device is warming up to 50 DEG C, tertiary carbonic acid glycidyl ester is added
Reaction kettle after mixing evenly, is added successively by monomers methyl methacrylate, n-butyl acrylate, acrylic acid adding apparatus
Semi-finished product, temperature are added the fluorine-containing polyester polysiloxane of terminal hydroxy group after rising to 70 DEG C, are stirring evenly and then adding into peroxidating trimethylacetic acid uncle
Butyl ester is removed under reduced pressure solvent, obtains acrylic resin modified after reacting 5h.
Graphene oxide modified polyurethane resin is prepared by weight by following raw material: 20 parts of graphite powder, persulfuric acid
6 parts of potassium, 20 parts of phosphorus pentoxide, 5 parts of potassium permanganate, 70 parts of sulfuric acid, 3% H2O2 20 parts, 3 parts of Silane coupling agent KH550 and
100 parts of polyaminoester emulsion.
Graphene oxide modified polyurethane resin is prepared by following methods:
S1. natural graphite powder, potassium peroxydisulfate and phosphorus pentoxide are weighed, is added to three mouthfuls equipped with sulfuric acid in the case of stirring
In flask, 3 h first are reacted in 60 DEG C of waters bath with thermostatic control, then three-necked flask is moved again in 25 DEG C of people of water bath with thermostatic control and reacts 5 h,
It filters, and cleans to neutrality with ionized water, dry in air, obtain pre-oxidation graphite；
S2. pre-oxidation graphite is weighed, is added in the three-necked flask equipped with sulfuric acid, is put into ice-water bath in the case of stirring,
After pre-oxidizing graphite and all dissolving, potassium permanganate is added, reacts 2 h, then three-necked flask is moved to 35 DEG C of people of water bath with thermostatic control
Middle reaction 40min, is eventually adding deionized water, continues 35 DEG C of 1 h of reaction, and 30% H is finally added dropwise2O2, so that there is no gases
Until generation, solution becomes glassy yellow, while hot centrifugal filtration, and is cleaned with a large amount of 5% hydrochloric acid and deionized water to neutrality, will
Final sediment is after the ultrasonic vibration of 1h, and dry 24 h obtain the graphite oxide of sheet at 90 DEG C in the culture dish of falling people
Alkene；
S3. the preparation of graphene oxide modified polyurethane resin: being warming up to 40 DEG C for reactor, and polyaminoester emulsion, oxidation is added
Graphene is stirring evenly and then adding into Silane coupling agent KH550, after reacting 3h, obtains graphene oxide modified polyurethane resin.
The preparation method of double-component aqueous road mark paint, comprising the following steps: sequentially add Organic fluoride by formula ratio
Acrylic resin modified, graphene oxide modified polyurethane resin, levelling agent BYK-381, dispersing agent C T-136 and organosilicon disappear
Infusion stirs evenly；Then coalescing agent is added, is ground after mixing evenly, until reaching regulation fineness, obtains two-component
Water-based road guide line coating.
Embodiment 3
Raw material form (parts by weight): 120 parts of organic fluorin modified crylic acid resin, 80 parts of graphene oxide modified polyurethane resin,
12 parts of coalescing agent, 6 parts of levelling agent BYK-381,4 parts of organic silicon defoamer and 3 parts of phenylethylene-maleic anhydride.Coalescing agent by
Following weight percent at being grouped as: antioxidant 6%, 800 mesh calcium powders 20%, adipate ester 14%, propylene glycol block polyether 15%,
Triethoxy octyl silane 10%, Tween-80 15% and Arlacel-80 10%.
Acrylic resin modified to be prepared by weight by following raw material: 35 parts of methyl methacrylate, acrylic acid are just
15 parts of butyl ester, 25 parts of acrylic acid, 17 parts of hydroxy-ethyl acrylate, 20 parts of isocyanates, 7 parts of the fluorine-containing polyester polysiloxane of terminal hydroxy group,
70 parts and 1 part of lauroyl peroxide of tertiary carbonic acid glycidyl ester.
It is acrylic resin modified to be prepared by following methods:
S1. hydroxy-ethyl acrylate and isocyanates are dissolved in dimethylbenzene, the polymerization inhibitor for accounting for isocyanates gross mass 0.1% is added
DNBP is heated to 70 DEG C of reaction 2h, obtains semi-finished product；
S2. ethyl acetate is added in a kettle, oil bath heating device is warming up to 50 DEG C, tertiary carbonic acid glycidyl ester is added
Reaction kettle after mixing evenly, is added successively by monomers methyl methacrylate, n-butyl acrylate, acrylic acid adding apparatus
Semi-finished product, temperature are added the fluorine-containing polyester polysiloxane of terminal hydroxy group after rising to 70 DEG C, are stirring evenly and then adding into lauroyl peroxide, instead
After answering 4h, solvent is removed under reduced pressure, obtains acrylic resin modified.
Graphene oxide modified polyurethane resin is prepared by weight by following raw material: 12 parts of graphite powder, persulfuric acid
4 parts of potassium, 12 parts of phosphorus pentoxide, 3 parts of potassium permanganate, 55 parts of sulfuric acid, 3% H2O2 12 parts, 1 part of Silane coupling agent KH550 and
70 parts of polyaminoester emulsion.
Graphene oxide modified polyurethane resin is prepared by following methods:
S1. natural graphite powder, potassium peroxydisulfate and phosphorus pentoxide are weighed, is added to three mouthfuls equipped with sulfuric acid in the case of stirring
In flask, 3 h first are reacted in 60 DEG C of waters bath with thermostatic control, then three-necked flask is moved again in 25 DEG C of people of water bath with thermostatic control and reacts 5 h,
It filters, and cleans to neutrality with ionized water, dry in air, obtain pre-oxidation graphite；
S2. pre-oxidation graphite is weighed, is added in the three-necked flask equipped with sulfuric acid, is put into ice-water bath in the case of stirring,
After pre-oxidizing graphite and all dissolving, potassium permanganate is added, reacts 2 h, then three-necked flask is moved to 35 DEG C of people of water bath with thermostatic control
Middle reaction 40min, is eventually adding deionized water, continues 35 DEG C of 1 h of reaction, and 30% H is finally added dropwise2O2, so that there is no gases
Until generation, solution becomes glassy yellow, while hot centrifugal filtration, and is cleaned with a large amount of 5% hydrochloric acid and deionized water to neutrality, will
Final sediment is after the ultrasonic vibration of 1h, and dry 24 h obtain the graphite oxide of sheet at 90 DEG C in the culture dish of falling people
Alkene；
S3. the preparation of graphene oxide modified polyurethane resin: being warming up to 40 DEG C for reactor, and polyaminoester emulsion, oxidation is added
Graphene is stirring evenly and then adding into Silane coupling agent KH550, after reacting 2h, obtains graphene oxide modified polyurethane resin.
The preparation method of double-component aqueous road mark paint, comprising the following steps: sequentially add Organic fluoride by formula ratio
Acrylic resin modified, graphene oxide modified polyurethane resin, levelling agent BYK-381, phenylethylene-maleic anhydride and organosilicon
Defoaming agent stirs evenly；Then coalescing agent is added, is ground after mixing evenly, until reaching regulation fineness, obtains double groups
Part water-based road guide line coating.
Embodiment 4
Raw material form (parts by weight): 130 parts of organic fluorin modified crylic acid resin, 110 parts of graphene oxide modified polyurethane resin,
18 parts of coalescing agent, 9 parts of levelling agent BYK-381, BYK0246 parts of defoaming agent and 5 parts of polyethylene glycol 400.Coalescing agent is by following
Weight percent at being grouped as: antioxidant 6%, 800 mesh calcium powders 20%, adipate ester 14%, propylene glycol block polyether 15%, three second
Oxygroup octyl silane 10%, Tween-80 15% and Arlacel-80 10%.
Acrylic resin modified to be prepared by weight by following raw material: 45 parts of methyl methacrylate, acrylic acid are just
25 parts of butyl ester, 45 parts of acrylic acid, 22 parts of hydroxy-ethyl acrylate, 25 parts of isocyanates, 9 parts of the fluorine-containing polyester polysiloxane of terminal hydroxy group,
2 parts of 80 parts of tertiary carbonic acid glycidyl ester and peroxidating trimethylacetic acid tertiary butyl ester.
It is acrylic resin modified to be prepared by following methods:
S1. hydroxy-ethyl acrylate and isocyanates are dissolved in dimethylbenzene, the polymerization inhibitor for accounting for isocyanates gross mass 0.1% is added
DNBP is heated to 70 DEG C of reaction 3h, obtains semi-finished product；
S2. ethyl acetate is added in a kettle, oil bath heating device is warming up to 50 DEG C, tertiary carbonic acid glycidyl ester is added
Reaction kettle after mixing evenly, is added successively by monomers methyl methacrylate, n-butyl acrylate, acrylic acid adding apparatus
Semi-finished product, temperature are added the fluorine-containing polyester polysiloxane of terminal hydroxy group after rising to 70 DEG C, are stirring evenly and then adding into potassium peroxydisulfate, react 5h
Afterwards, solvent is removed under reduced pressure, obtains acrylic resin modified.
Graphene oxide modified polyurethane resin is prepared by weight by following raw material: 18 parts of graphite powder, persulfuric acid
6 parts of potassium, 17 parts of phosphorus pentoxide, 5 parts of potassium permanganate, 65 parts of sulfuric acid, 3% H2O2 18 parts, 2 parts of Silane coupling agent KH550 and
80 parts of polyaminoester emulsion.
Graphene oxide modified polyurethane resin is prepared by following methods:
S1. natural graphite powder, potassium peroxydisulfate and phosphorus pentoxide are weighed, is added to three mouthfuls equipped with sulfuric acid in the case of stirring
In flask, 3 h first are reacted in 60 DEG C of waters bath with thermostatic control, then three-necked flask is moved again in 25 DEG C of people of water bath with thermostatic control and reacts 5 h,
It filters, and cleans to neutrality with ionized water, dry in air, obtain pre-oxidation graphite；
S2. pre-oxidation graphite is weighed, is added in the three-necked flask equipped with sulfuric acid, is put into ice-water bath in the case of stirring,
After pre-oxidizing graphite and all dissolving, potassium permanganate is added, reacts 2 h, then three-necked flask is moved to 35 DEG C of people of water bath with thermostatic control
Middle reaction 40min, is eventually adding deionized water, continues 35 DEG C of 1 h of reaction, and 30% H is finally added dropwise2O2, so that there is no gases
Until generation, solution becomes glassy yellow, while hot centrifugal filtration, and is cleaned with a large amount of 5% hydrochloric acid and deionized water to neutrality, will
Final sediment is after the ultrasonic vibration of 1h, and dry 24 h obtain the graphite oxide of sheet at 90 DEG C in the culture dish of falling people
Alkene；
S3. the preparation of graphene oxide modified polyurethane resin: being warming up to 40 DEG C for reactor, and polyaminoester emulsion, oxidation is added
Graphene is stirring evenly and then adding into Silane coupling agent KH550, after reacting 3h, obtains graphene oxide modified polyurethane resin.
The preparation method of double-component aqueous road mark paint, comprising the following steps: sequentially add Organic fluoride by formula ratio
Acrylic resin modified, graphene oxide modified polyurethane resin, levelling agent BYK-381, polyethylene glycol 400 and defoaming agent
BYK024 is stirred evenly；Then coalescing agent is added, is ground after mixing evenly, until reaching regulation fineness, obtains double groups
Part water-based road guide line coating.
Embodiment 5
Raw material form (parts by weight): 125 parts of organic fluorin modified crylic acid resin, 95 parts of graphene oxide modified polyurethane resin,
16 parts of coalescing agent, 7 parts of levelling agent BYK-381,5 parts of GPE type defoaming agent and 4 parts of hexenyl bis-stearamides.Coalescing agent by
Following weight percent at being grouped as: antioxidant 6%, 800 mesh calcium powders 20%, adipate ester 14%, propylene glycol block polyether 15%,
Triethoxy octyl silane 10%, Tween-80 15% and Arlacel-80 10%.
Acrylic resin modified to be prepared by weight by following raw material: 40 parts of methyl methacrylate, acrylic acid are just
20 parts of butyl ester, 30 parts of acrylic acid, 20 parts of hydroxy-ethyl acrylate, 25 parts of isocyanates, 8 parts of the fluorine-containing polyester polysiloxane of terminal hydroxy group,
75 parts and 1.5 parts of peroxidized t-butyl perbenzoate of tertiary carbonic acid glycidyl ester.
It is acrylic resin modified to be prepared by following methods:
S1. hydroxy-ethyl acrylate and isocyanates are dissolved in dimethylbenzene, the polymerization inhibitor for accounting for isocyanates gross mass 0.1% is added
DNBP is heated to 70 DEG C of reaction 2.5h, obtains semi-finished product；
S2. ethyl acetate is added in a kettle, oil bath heating device is warming up to 50 DEG C, tertiary carbonic acid glycidyl ester is added
Reaction kettle after mixing evenly, is added successively by monomers methyl methacrylate, n-butyl acrylate, acrylic acid adding apparatus
Semi-finished product, temperature are added the fluorine-containing polyester polysiloxane of terminal hydroxy group after rising to 70 DEG C, are stirring evenly and then adding into ammonium persulfate, react
After 4.5h, solvent is removed under reduced pressure, obtains acrylic resin modified.
Graphene oxide modified polyurethane resin is prepared by weight by following raw material: 16 parts of graphite powder, persulfuric acid
5 parts of potassium, 15 parts of phosphorus pentoxide, 4 parts of potassium permanganate, 60 parts of sulfuric acid, 3% H2O2 15 parts, 1.5 parts of Silane coupling agent KH550
With 75 parts of polyaminoester emulsion.
Graphene oxide modified polyurethane resin is prepared by following methods:
S1. natural graphite powder, potassium peroxydisulfate and phosphorus pentoxide are weighed, is added to three mouthfuls equipped with sulfuric acid in the case of stirring
In flask, 3 h first are reacted in 60 DEG C of waters bath with thermostatic control, then three-necked flask is moved again in 25 DEG C of people of water bath with thermostatic control and reacts 5 h,
It filters, and cleans to neutrality with ionized water, dry in air, obtain pre-oxidation graphite；
S2. pre-oxidation graphite is weighed, is added in the three-necked flask equipped with sulfuric acid, is put into ice-water bath in the case of stirring,
After pre-oxidizing graphite and all dissolving, potassium permanganate is added, reacts 2 h, then three-necked flask is moved to 35 DEG C of people of water bath with thermostatic control
Middle reaction 40min, is eventually adding deionized water, continues 35 DEG C of 1 h of reaction, and 30% H is finally added dropwise2O2, so that there is no gases
Until generation, solution becomes glassy yellow, while hot centrifugal filtration, and is cleaned with a large amount of 5% hydrochloric acid and deionized water to neutrality, will
Final sediment is after the ultrasonic vibration of 1h, and dry 24 h obtain the graphite oxide of sheet at 90 DEG C in the culture dish of falling people
Alkene；
S3. the preparation of graphene oxide modified polyurethane resin: being warming up to 40 DEG C for reactor, and polyaminoester emulsion, oxidation is added
Graphene is stirring evenly and then adding into Silane coupling agent KH550, after reacting 2.5h, obtains graphene oxide modified polyurethane resin.
The preparation method of double-component aqueous road mark paint, comprising the following steps: sequentially add Organic fluoride by formula ratio
Acrylic resin modified, graphene oxide modified polyurethane resin, levelling agent BYK-381, hexenyl bis-stearamides and GPE type
Defoaming agent stirs evenly；Then coalescing agent is added, is ground after mixing evenly, until reaching regulation fineness, obtains double groups
Part water-based road guide line coating.
Comparative example 1
Compared with Example 5, organic fluorin modified crylic acid resin replaces with conventional propylene acid resin.
Comparative example 2
Compared with Example 5, graphene oxide modified polyurethane resin replaces with common polyurethane resin.
Comparative example 3
Compared with Example 5, coalescing agent is not added.
Test case 1
By 1-5 of the embodiment of the present invention, comparative example 1-3 and commercially available double-component aqueous road mark paint progressive according to national standards
It can test, the results are shown in Table 1.
Table 1
As seen from the above table, the double-component aqueous road mark paint of 1-5 of embodiment of the present invention preparation has similar comprehensive performance,
Its performance test ratio and commercial like product are more excellent.Compared with comparative example 1, using its mechanics of the coating of conventional propylene acid resin
Performance decline, water resistance and resistance to soiling are decreased obviously；Compared with comparative example 2, had using the coating of common polyurethane resin
Poor mechanical property, wearability are poor；Compared with comparative example 3, wearability, mechanical property of the coalescing agent for coating are added
Preferably improve Deng having.
Compared with prior art, the present invention uses organic fluorinated silicone compound and tertiary carbonic acid glycidyl ester modified acroleic acid tree
Rouge, wherein Organic fluoride, organic-silicon-modified acrylic resin can significantly improve the water-fast, resistance to of the coating of acrylic resin formation
Dirt, tertiary carbonic acid glycidyl ester is the active solvent of the synthetic resin in acrylic resin, acrylic resin modified at this
In synthesis, without adding solvent, its safety and environmental protection performance is improved, simultaneously as the steric effect of tertiary carbonic acid glycidyl ester, makes
Obtaining final resin, there is good acid resistance to improve the gloss retention of coating moreover, it is insensitive to UV；Using graphite oxide
Alkene modified polyurethane resin can significantly improve the mechanical property and wear-resisting property of polyurethane resin；
Paint film toughness and intensity are improved using adipate ester；It is not volatile using propylene glycol block polyether, it can dissolve in paint
Fine oxide crystallization in pigments and fillers prevents it from forming the structure reduction paint film intensity for destroying paint film；It is pungent using triethoxy
Surface of the paint film smoothness can be improved in base silane, not only promotes paint film appearance, and it is wear-resisting also to can reduce the coarse raising of surface of the paint film
Performance；The ageing-resistant performance of coating is improved using antioxidant；Adding surfactant reduces the surface tension of coating, and it is viscous to enhance it
Attached property；
Preparation method of the present invention is simple, and coating obtained is water paint, has the good feature of environmental protection, low VOC emission, and make
The coating obtained has good gloss retention, water-fast, acidproof, chemical corrosion resistance, and film forming is quickly and fine and smooth uniform, has after film forming
Preferable intensity and mechanical property, have broad application prospects.
Those skilled in the art is not under conditions of departing from the spirit and scope of the present invention that claims determine, also
Various modifications can be carried out to the above content.Therefore the scope of the present invention is not limited in above explanation, but by
The range of claims determines.
Claims (10)
1. a kind of double-component aqueous road mark paint, which is characterized in that be prepared from the following materials: Organic fluoride modified propylene
Acid resin, graphene oxide modified polyurethane resin, coalescing agent, levelling agent BYK-381, defoaming agent and dispersing agent；
It is described acrylic resin modified to be prepared from the following materials: methyl methacrylate, n-butyl acrylate, acrylic acid,
The fluorine-containing polyester polysiloxane of hydroxy-ethyl acrylate, isocyanates, terminal hydroxy group, tertiary carbonic acid glycidyl ester and initiator；
The initiator is selected from peroxidized t-butyl perbenzoate, peroxidating trimethylacetic acid tertiary butyl ester, isopropyl benzene hydroperoxide, tertiary fourth
One of base hydrogen peroxide, benzoyl peroxide, lauroyl peroxide, potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate are several
Kind；
The graphene oxide modified polyurethane resin is prepared from the following materials: graphite powder, potassium peroxydisulfate, five oxidations two
Phosphorus, potassium permanganate, sulfuric acid, 3% H2O2, Silane coupling agent KH550 and polyaminoester emulsion.
2. a kind of double-component aqueous road mark paint according to claim 1, which is characterized in that by weight by following raw material
Part be prepared: organic fluorin modified crylic acid resin 100-150 parts, 70-120 parts of graphene oxide modified polyurethane resin, at
10-20 parts of film auxiliary agent, 5-10 parts of levelling agent BYK-381,3-7 parts of defoaming agent and 2-5 parts of dispersing agent；
It is described acrylic resin modified to be prepared by weight by following raw material: 30-50 parts of methyl methacrylate, acrylic acid
10-30 parts of N-butyl, 20-50 parts of acrylic acid, 15-25 parts of hydroxy-ethyl acrylate, 20-30 parts of isocyanates, terminal hydroxy group are fluorine-containing poly-
5-10 parts of ester polysiloxanes, 50-100 parts of tertiary carbonic acid glycidyl ester and 1-3 parts of initiator；
The graphene oxide modified polyurethane resin is prepared by weight by following raw material: 10-20 parts of graphite powder, over cure
Sour potassium 3-6 parts, 10-20 parts of phosphorus pentoxide, 2-5 parts of potassium permanganate, 50-70 parts of sulfuric acid, 3% H2O2 10-20 parts, silane idol
Join 1-3 parts and polyaminoester emulsion 50-100 parts of agent KH550.
3. a kind of double-component aqueous road mark paint according to claim 2, which is characterized in that by weight by following raw material
Part be prepared: organic fluorin modified crylic acid resin 120-130 parts, 80-110 parts of graphene oxide modified polyurethane resin, at
12-18 parts of film auxiliary agent, 6-9 parts of levelling agent BYK-381,4-6 parts of defoaming agent and 3-5 parts of dispersing agent；
It is described acrylic resin modified to be prepared by weight by following raw material: 35-45 parts of methyl methacrylate, acrylic acid
15-25 parts of N-butyl, 25-45 parts of acrylic acid, 17-22 parts of hydroxy-ethyl acrylate, 20-25 parts of isocyanates, terminal hydroxy group are fluorine-containing poly-
7-9 parts of ester polysiloxanes, 70-80 parts of tertiary carbonic acid glycidyl ester and 1-2 parts of initiator；
The graphene oxide modified polyurethane resin is prepared by weight by following raw material: 12-18 parts of graphite powder, over cure
Sour potassium 4-6 parts, 12-17 parts of phosphorus pentoxide, 3-5 parts of potassium permanganate, 55-65 parts of sulfuric acid, 3% H2O2 12-18 parts, silane idol
Join 1-2 parts and polyaminoester emulsion 70-80 parts of agent KH550.
4. a kind of double-component aqueous road mark paint according to claim 3, which is characterized in that by weight by following raw material
Part is prepared: 125 parts of organic fluorin modified crylic acid resin, 95 parts of graphene oxide modified polyurethane resin, coalescing agent 16
Part, 7 parts of levelling agent BYK-381,5 parts of defoaming agent and 4 parts of dispersing agent；
Described acrylic resin modified to be prepared by weight by following raw material: 40 parts of methyl methacrylate, acrylic acid are just
20 parts of butyl ester, 30 parts of acrylic acid, 20 parts of hydroxy-ethyl acrylate, 25 parts of isocyanates, 8 parts of the fluorine-containing polyester polysiloxane of terminal hydroxy group,
75 parts and 1.5 parts of initiator of tertiary carbonic acid glycidyl ester；
The graphene oxide modified polyurethane resin is prepared by weight by following raw material: 16 parts of graphite powder, persulfuric acid
5 parts of potassium, 15 parts of phosphorus pentoxide, 4 parts of potassium permanganate, 60 parts of sulfuric acid, 3% H2O2 15 parts, 1.5 parts of Silane coupling agent KH550
With 75 parts of polyaminoester emulsion.
5. a kind of double-component aqueous road mark paint according to claim 1, which is characterized in that the modified acroleic acid tree
Rouge is prepared by following methods:
S1. hydroxy-ethyl acrylate and isocyanates are dissolved in dimethylbenzene, the polymerization inhibitor for accounting for isocyanates gross mass 0.1% is added
DNBP is heated to 70 DEG C of reaction 2-3h, obtains semi-finished product；
S2. ethyl acetate is added in a kettle, oil bath heating device is warming up to 50 DEG C, tertiary carbonic acid glycidyl ester is added
Reaction kettle after mixing evenly, is added successively by monomers methyl methacrylate, n-butyl acrylate, acrylic acid adding apparatus
Semi-finished product, temperature are added the fluorine-containing polyester polysiloxane of terminal hydroxy group after rising to 70 DEG C, are stirring evenly and then adding into initiator, react 4-5h
Afterwards, solvent is removed under reduced pressure, obtains acrylic resin modified.
6. a kind of double-component aqueous road mark paint according to claim 1, which is characterized in that the graphene oxide changes
Property polyurethane resin is prepared by following methods:
S1. natural graphite powder, potassium peroxydisulfate and phosphorus pentoxide are weighed, is added to three mouthfuls equipped with sulfuric acid in the case of stirring
In flask, 3 h first are reacted in 60 DEG C of waters bath with thermostatic control, then three-necked flask is moved again in 25 DEG C of people of water bath with thermostatic control and reacts 5 h,
It filters, and cleans to neutrality with ionized water, dry in air, obtain pre-oxidation graphite；
S2. pre-oxidation graphite is weighed, is added in the three-necked flask equipped with sulfuric acid, is put into ice-water bath in the case of stirring,
After pre-oxidizing graphite and all dissolving, potassium permanganate is added, reacts 2 h, then three-necked flask is moved to 35 DEG C of people of water bath with thermostatic control
Middle reaction 40min, is eventually adding deionized water, continues 35 DEG C of 1 h of reaction, and 30% H is finally added dropwise2O2, so that there is no gases
Until generation, solution becomes glassy yellow, while hot centrifugal filtration, and is cleaned with a large amount of 5% hydrochloric acid and deionized water to neutrality, will
Final sediment is after the ultrasonic vibration of 1h, and dry 24 h obtain the graphite oxide of sheet at 90 DEG C in the culture dish of falling people
Alkene；
S3. the preparation of graphene oxide modified polyurethane resin: being warming up to 40 DEG C for reactor, and polyaminoester emulsion, oxidation is added
Graphene is stirring evenly and then adding into Silane coupling agent KH550, after reacting 2-3h, obtains graphene oxide modified polyurethane resin.
7. a kind of double-component aqueous road mark paint according to claim 1, which is characterized in that the dispersing agent selects oneself
Alkenyl bis-stearamides, glyceryl monostearate, glyceryl tristearate, polycarboxylic acids ammonium salt, sodium acrylate salt copolymer, poly- second
One or more of glycol 200, polyethylene glycol 400, phenylethylene-maleic anhydride and CT-136.
8. a kind of double-component aqueous road mark paint according to claim 1, which is characterized in that the defoaming agent is selected from
One or more of GPE type defoaming agent, organic silicon defoamer and BYK024.
9. a kind of double-component aqueous road mark paint according to claim 1, which is characterized in that the coalescing agent includes
Antioxidant, 800 mesh calcium powders, adipate ester, propylene glycol block polyether, triethoxy octyl silane, Tween-80 and Arlacel-80.
10. a kind of method for preparing the double-component aqueous road mark paint as described in any one of claim 1-9 claim,
It is characterized in that, comprising the following steps: sequentially add the modified poly- ammonia of organic fluorin modified crylic acid resin, graphene oxide by formula ratio
Ester resin, levelling agent BYK-381, dispersing agent and defoaming agent, stir evenly；Then coalescing agent is added, carries out after mixing evenly
Grinding obtains double-component aqueous road mark paint until reaching regulation fineness.
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Application publication date: 20191108 |